US20130180913A1 - Water filtration system using hybrid nano carbon, silver, iron and aluminium oxide - Google Patents

Water filtration system using hybrid nano carbon, silver, iron and aluminium oxide Download PDF

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US20130180913A1
US20130180913A1 US13/791,058 US201313791058A US2013180913A1 US 20130180913 A1 US20130180913 A1 US 20130180913A1 US 201313791058 A US201313791058 A US 201313791058A US 2013180913 A1 US2013180913 A1 US 2013180913A1
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Prior art keywords
water
filter
carbon
silver
alumina
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US13/791,058
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Sabyasachi Sarkar
Abdul Allam
Afreen Allam
Iffat Allam
Arsheen Allam
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CNanoz Inc
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CNanoz Inc
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Priority claimed from US13/181,855 external-priority patent/US20120012522A1/en
Application filed by CNanoz Inc filed Critical CNanoz Inc
Priority to US13/791,058 priority Critical patent/US20130180913A1/en
Assigned to CNANOZ INC reassignment CNANOZ INC ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ALLAM, ARSHEEN, ALLAM, AFREEN, ALLAM, ABDUL, ALLAM, IFFAT, SARKAR, SABYASACHI, DR.
Priority to CN201310218809.7A priority patent/CN104028044A/en
Publication of US20130180913A1 publication Critical patent/US20130180913A1/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/02Loose filtering material, e.g. loose fibres
    • B01D39/06Inorganic material, e.g. asbestos fibres, glass beads or fibres
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055Carbonaceous material
    • B01D39/2058Carbonaceous material the material being particulate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039Inorganic membrane manufacture
    • B01D67/0067Inorganic membrane manufacture by carbonisation or pyrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
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    • B01D69/12Composite membranes; Ultra-thin membranes
    • B01D69/1216Three or more layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02Inorganic material
    • B01D71/021Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02Inorganic material
    • B01D71/024Oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/2803Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28052Several layers of identical or different sorbents stacked in a housing, e.g. in a column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204Inorganic carriers, supports or substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234Inorganic material layers
    • B01J20/3236Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/318Preparation characterised by the starting materials
    • C01B32/324Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/0258Types of fibres, filaments or particles, self-supporting or supported materials comprising nanoparticles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10Filtering material manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2323/00Details relating to membrane preparation
    • B01D2323/46Impregnation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/103Arsenic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • C02F2101/14Fluorine or fluorine-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/005Processes using a programmable logic controller [PLC]
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/08Nanoparticles or nanotubes

Definitions

  • the present invention relates to the production of carbon nanospheres and to use of the nanospheres in water filters and methods of filtering water using the composition in a water filter device.
  • a number of methods have been developed to filter or otherwise remove pollutants and unwanted elements from drinking water. Included are methods of precipitation, ceramic or other filters, calcium or magnesium hydroxide, activated carbon, nano silver, chemical reaction, and the like. These materials are frequently used for incorporation as filter material in a filter device such as a housing containing filter material where water can be passed through for filtration purposes. The size of the particle filtered out is directly related to the porosity of the filtering material. Filtration of water is typically divided into nano porous, meso porous, micro porous, and the like.
  • the present invention provides novel filtration material that is cost effective and environmentally friendly, and filtration devices made from those materials.
  • the materials are porous materials that can be used in water filtration devices and to filter other liquids.
  • the porous nanospheres, the nanospheres with carboxyl groups and/or with metallated carboxy groups can each together or separate be effective in not only filtering water for particulate matter, but in the case of the metallated nanospheres, binding and thus removing arsenic and fluoride and other materials from water passed through such filter material.
  • This combined with ferrice oxide or alumina impregnated with ferric oxide overcomes many of the prior art problems with water filtration.
  • the present invention relates to a water filtering device comprising:
  • FIG. 1 depicts water soluble carbon nanospheres (CNSs) showing D and G band with mixing of overtones around 2700 cm ⁇ 1 in Raman Spectrum.
  • FIG. 2 is an EDX spectra of CNSs showing the presence of only carbon and oxygen.
  • FIG. 3 is a SEM Image of pure Carbon Nanospheres.
  • FIG. 4 is a TEM image of Carbon Nanospheres.
  • FIG. 5 is a HRTEM image of CNSs showing sizes of the nanospheres with onion type multilayered concentric nanospheres.
  • FIG. 6 is a SEM image of the carboxylated CNSs showing size and shape.
  • FIG. 7 is a SEM image of carboxy metallated CNSs showing sizes of the nanospheres.
  • FIG. 8 is a pictorial representation of the metallation of carboxylated carbon nanosphere.
  • FIG. 9 is a representation of a filter of the present invention.
  • FIG. 10 is a representation of an alternate embodiment of a filter of the present invention.
  • FIG. 11 is a relationship drawing of a microcontroller with filters of the present invention.
  • the terms “a” or “an”, as used herein, are defined as one or as more than one.
  • the term “plurality”, as used herein, is defined as two or as more than two.
  • the term “another”, as used herein, is defined as at least a second or more.
  • the terms “including” and/or “having”, as used herein, are defined as comprising (i.e., open language).
  • the term “coupled”, as used herein, is defined as connected, although not necessarily directly, and not necessarily mechanically.
  • filtration As used herein the terms and phrases “filtration”, “filtration of water”, “water filtering device” and “water filter” refer to material/devices that can be utilized to filter a liquid such as water and remove certain contaminants.
  • the material can be placed/positioned in a filtration device such as a water filter and liquid passed through one or more layers of the filtration material in the normal manner for water filtration.
  • the material can be shaped, placed, containerized, or the like as needed to filter water under gravity pressure or other forced pressure.
  • liquids other than water that are compatible with carbon filtration material can also be filtered.
  • nanospheres refers to concentric spherical carbon structures, granules and the like which outermost spheres are in the size range of about 25 nm to about 50 nm that are isolated from the pyrolytic combustion of a carbonaceous material.
  • the pyrolytic combustion produces concentric spheres that are two or more spheres inside another (see FIG. 8 ).
  • the nanospheres When collected in a container in quantity (such as being placed in a filter), the nanospheres fill a given space like marbles fill a container, creating the minimal amount of space possible and aligning themselves due to their spherical shape.
  • the porosity of the material is derived by spaces in-between the spheres since there is a consistent size of that space when packing spherical objects.
  • the space between the spheres can be adjusted, that is, made smaller, thus filtering smaller particles by placing addition groups on the surface of the spheres, thus making them fuzzy and thus taking up space in the space between the spheres.
  • the present invention includes carboxylation of the spheres wherein carboxylation is obtained by oxidation of the spheres. Greater carboxylation of the spheres requires the spheres to remain in contact with the oxidizing agent (such as nitric acid) for a longer period.
  • the carboxylation once it reaches a certain point, makes the spheres water soluble, therefore, in the case where they are to be utilized for water filtration, the carboxylation should be kept below an amount that makes them soluble in the water being filtered. That amount can easily be determined by varying the oxidation time and testing a batch. Where a fluid other than water is being filtered, the amount of carboxylation can be less important.
  • the carboxylate groups can also be metallated. Metallation will cause the spheres to be non-water soluble so, in that instance as much carboxylation as desired can be done.
  • the non substituted spheres and these substituted spheres can be mixed together in any combination desired depending on the porosity desired. The more substitutions, the smaller the spaces and the smaller the particle that is filtered out by the material.
  • the material is loosely packed and can be placed in a cartridge or other container to hold it in place during the filtration process.
  • a binder can be utilized to make the spheres sticky enough to hold together as a composite.
  • a silicic acid solution could coat the spheres without decreasing significantly the porosity of the material.
  • Other binders such as low density polyethylene or ethyl vinyl acetate, could be determined by one skilled in the art.
  • not carboxylated sufficiently to cause the carbon nano spheres to be water soluble refers to only oxidizing the spheres enough so that the resulting spheres are still not soluble in water to a significant degree.
  • metal ion As used herein the terms “metal ion”, “metallate”, “metallation”, and “metallated” refer to treating the carboxylate groups' place on the nanospheres to place a metal ion on the group in place of the carboxylic group, i.e. replacing —COON with —COM wherein M is the metal ion.
  • Metal ions can be selected from metals in the transition metals and poor metal groups from the periodic table. For example, iron, silver, and aluminum could be selected.
  • the ions can be delivered in the form of the ion or a salt which dissociates to deliver the metal ion.
  • certain ions can bind compounds and the selection of the metal ion can be done to selectively bind certain compounds dissolved in the liquid such as water in addition to filtering the media.
  • the liquid such as water
  • silver is known to attach to bacteria binding it, and in other cases actually killing it.
  • Iron and aluminum can bind arsenic and fluoride respectively and can similarly be utilized.
  • One skilled in the art can determine which metal to select based on binding capacity, cost, ease of use, and the like.
  • a “carbonaceous material” refers to material which when pyrolyzed, can form carbonaceous nanospheres (about 25 nm to about 50 nm in size).
  • the carbonaceous material is an organic material that is a material that was living such as animal or plant material.
  • the material could be a cellulosic material, wood, coconut shell, wood wool, wood dust, or the like.
  • Other materials can also be utilized which can be pyrolyzed in sufficient quantity to make enough spheres to make a filter.
  • oxidizing agent refers to a composition that can oxidize the surface of a carbon sphere to produce carboxylic acid groups on the surface, for example concentrated or diluted nitric acid; though there is damage to the spheres the more concentrated the acid is.
  • activated carbon with silver nitrate refers to carbon granules which have adsorbed onto it silver nitrate for the purpose of inhibiting growth of bacteria.
  • 0.2 milligrams of silver nitrate is dissolved in one liter of “distilled water” to prepare a 2 ppm (parts per million) solution.
  • About 2 kilograms of carboxylated activated carbon granules are soaked in the 2 ppm silver nitrate solution for 1-2 hours. This soaked mass is dried in sun rays and then heated to 180° C. which results in impregnating the activated carbon with metallic silver.
  • Silver nitrate is photo decomposed and finally thermally decomposed and metallic silver is impregnated to the entire mass of the nano carbon carboxylate.
  • This carboxylated activated carbon impregnated with silver in this form prevents/retards any bacteria biofilm formation.
  • activated alumina is aluminum hydroxide made by dehydroxylating it in a way that produces a highly porous material.
  • 10% (of alumina weight) ferrous sulphate solution in 50-150 mL water, is added to alumina granules (size 0.5-2 mm) and mixed well gently.
  • 10% ammonia solution is added until the pH of the supernatant becomes 6-7.
  • the alumina granules turn green. These green granules are left in the air and shaken well for auto-oxidation in atmospheric air. As a result, the green colored granules turn an orange-red color.
  • orange-red alumina granules are heated up to and kept at 400° C. in a furnace for 1 hour. Then the furnace is allowed to cool at room temperature. Now the orange-red alumina is ready to be used as an adsorbent for fluoride and arsenic present in the water.
  • the filter can be combined with a microcontroller.
  • the microcontroller can control if water passes through the filter or if the filter needs changing. So, for example, if a filter needs changing, the filter could be shut off.
  • the filter is digitally identified by the microcontroller so once the filter is used up, the microcontroller will never let it be used again preventing reuse of spent filters or use beyond useful life.
  • Concentric carbon nanospheres are prepared by the pyrolysis of carbonaceous material under insufficient air.
  • the carbonaceous material can be any material capable of pyrolysis (600 to 850° C.) that produces nanospheres but in one embodiment is a natural material such as a biologic animal or plant material. Examples include but are not limited to coconut shell, wood wool, and wood dust. It can also include cellulose materials and wood.
  • fire/heat is applied to the carbonaceous material in a confined chamber under the flow of blowing air where the carbonaceous matter is allowed to glow.
  • An outlet on the top of the chamber continuously ejects the distillation byproducts such as ligneous acid under the flow of air from the bottom of the chamber maintained at a temperature around 600-850° C. The process takes several hours and is dependent on the quantity of the feed stock.
  • water is slowly introduced by sprinkling and the steam produced is dispersed or removed along with the residual byproduct. The residual mass is also cooled down.
  • the mass is leached with alcohol to remove traces of soluble organic byproduct, especially products like ligneous acid which can be trapped in the pores (spaces between the spheres) and air dried. It can also be washed with 10% sodium hydroxide solution for that purpose.
  • the dried mass is pulverized to get the desired size of pieces containing multiple carbon nano spheres (macro sized, in the millimeter range) by using appropriate mesh size while the individual spheres are together as shown in the SEM photographs.
  • the CNS is now ready for further derivitization processes like carboxylation followed by metallation or can be utilized as is as a filtration material.
  • the collected black material from pyrolysis of the carbonaceous material which comprises amorphous carbon and carbon nanospheres is purified by washing.
  • biomass acid and other impurities are removed by washing with a solution of 10% sodium hydroxide.
  • This can then be subjected to a first derivitization by treating it with an oxidizing agent such as nitric acid to introduce multiple carboxylic acid groups on the surfaces of the CNS. The longer the spheres are oxidized, the greater the carboxylization.
  • the carboxylated derivatized CNS are treated under sonication in water and are subjected to a second derivitization by adding metal ions such as ferric ion and aluminum ion and by adjusting the pH to metallate at least a portion of the carboxylic acid groups.
  • the formation can occur with the addition of ammonia followed by drying the mixture to a dried residue. Appropriate mixing and drying is done at each step. In most cases, what remains is a combination of spheres that are carboxylated, some that are metallated or a combination of the two. Non-deritivized spheres may remain as well.
  • the filter material can contain any combination of the three types of nanospheres either because they all exist during producing them or because they are made separately and combined.
  • the concentration of metal to CNS can vary from about 0.2% to about 10% by weight (of total CNS weight).
  • the resultant mass is washed with water to remove free metal ions and other counter ions and heated to around 100° C. to yield the metal impregnated form of CNS. See FIG. 8 for example. All these forms are activated carbon with assorted porosity.
  • the material of the present invention can then be placed in a container or otherwise contained or formed as necessary for the desired filtration purpose or filter or filter holder.
  • the shape can be as needed, for example to be placed in the flow of water to be filtered either by gravity or pressure filtration.
  • it can be contained in a standard filter holder or the like or custom holders for inline use can be created and such are unlimited in variety and shape.
  • thinner filters can be utilized, up to 8 inches, depending on how much must be filtered out.
  • virtually any thickness can be utilized as long as the pressure is not so great as to damage the filter material of the present invention.
  • CNS When CNS are prepared from low cost material, it can be utilized to develop eco-friendly filters that trap or bind soluble compounds of toxic metal ions and anions, pathogens and virus, and industrial organic molecules like pesticides and aromatic hydrocarbons as well as color and odor in a unique integrated manner.
  • the filter material of the present invention is also capable of reducing the salinity of water.
  • the advantage of this invention over the comparable inventions lies on the following: the proposed system can remove inorganic, organic and bio related toxic materials commonly available in water to make the water safe for drinking purposes.
  • the proposed system also requires no energy input as normally needed in systems that use ozone, ultraviolet radiation, chlorination, or reverse osmosis to remove pathogens and virus.
  • the composition traps these pathogens in the pores and surface of CNS without need for any energy input.
  • the filter material which has bound materials such as arsenic and fluoride and bacteria to it can be chemically treated to regenerate the material.
  • it because of the low cost involved in the manufacturing of the material, it can be readily disposed of or used as crude carbonaceous fuel if it no longer filters sufficiently for filtration utilization.
  • silver impregnated nano carbon granules with either ferric oxide impregnated alumina globules or ferric oxide globules or both are added with 5-10% of the binder such as polypropylene or polyethylene (high or low density) powder.
  • the binder such as polypropylene or polyethylene (high or low density) powder.
  • These are mixed thoroughly and placed in cylindrical shaped molds. Pressure is applied to the top surface of the mixed powder in the mold along with application of heat to the metallic mold in order to bring the temperature up to the melting point of the organic binder (i.e polypropylene, polyethylene or any other binder). After a few minutes, the heating is stopped to allow the composite material to shrink/contract. After a couple of hours, when the mold is cooled off, the cylindrical cartridge which is now in solid form is removed and is ready for use as a filter.
  • the binder such as polypropylene or polyethylene (high or low density) powder.
  • the silver impregnated nano carbon with ferric oxide coated alumina in a particular ratio depending on the level of fluoride or arsenic in the water in a specific area. Cylindrical shape of this composite mixture is created as described above. In select areas where water contains predominantly fluoride, the alumina globules will be used along with the silver impregnated nano carbon granules. In areas where water contains predominantly Arsenic, then ferric oxide globules activated by heating to about 400° C., will be used along with the silver impregnated nano carbon granules.
  • alumina treated with nano ferric oxide along with silver impregnated nano carbon granules will be used.
  • arsenic and fluoride are present in water, then alumina globules and ferric oxide globules will be used proportionately depending on which (arsenic or alumina) has higher content.
  • Silver impregnated nano carbon granules will be used as well.
  • the relative variation in ratios of the silver impregnated nano carbon to ferric coated alumina and ferric oxide globules will provide varied version of filter cartridges dependent on the need based on the quality of water. If just (a) organic molecules such as petroleum products, pesticides, herbicides (b) microbes, pathogenic coli, viruses and (c) heavy metals like mercury or cadmium or lead are present in the water, then the activated nano carbon alone is effective. If the water is contaminated with fluoride as well, then a proportionate amount of ferric treated alumina is required in the cartridges.
  • ferric oxide granules is included along with the silver impregnated carbon in the hybrid filtration cartridge.
  • Filter material binded with the help of binders such as polypropylene and polyethylene increase the contact time of water as it passes through the cylindrical wall of the compressed hybrid carbon nano filter. This enhances the performance of filtration compared with filter material in the loose granular format.
  • the filter 1 consists of the following horizontal layers. Unfiltered water enters the top 2 of the filter 1 and encounters the top most layer 5 of the filter which consists of silver impregnated carbon nano.
  • the pesticides middle layer 4 consists of activated alumina treated with ferric oxide, activated alumina globules, or ferric oxide globules, depending on the presence of fluoride and or arsenic and their levels in water to be filtered.
  • the last layer 3 consists of Calcium Bentonite and Somelite to remove any traces of bacteria, toxins and heavy metals. In addition, this last layer helps to enhance the taste of water.
  • filtered water 6 is removed from the bottom of the filter.
  • the filter may be of any convenient size.
  • the treated carbon material and ferric oxide impregnated alumina or ferric oxide globule may be separately placed in different partitions (this is done to get the carbon regenerated readily after use). In one embodiment, it may work as follows:
  • the carbon and alumina can be regenerated and reused (recycling).
  • the filter removes bacteria as well as fluoride and arsenic (more fluoride removal than a conventional system).
  • the cartridge When making a small version of the gravity filter, once used, the cartridge can be discarded, and depending on the need of cartridge, one can use only carbon or carbon with alumina treated with ferric oxide or carbon with ferric oxide or carbon with both alumina and ferric oxide.
  • a tap filter (one that can attach to a faucet or the like is shown in FIG. 10 ).
  • the parts and layers have the indicated materials but the water to be filtered 2 enters the center of the filter and is pushed horizontally by the pressure of the flow of water to produce filtered water 6 on the outside of the filter. It also removes bacteria, other toxic organic and biological contaminants, toxic heavy metals as well as fluoride and arsenic (more fluoride removal than conventional system). It is small and portable and requires only overhead tank water pressure operative even on the top most floor of a building. Replacement of cartridges will be indicated with flashing indicator light (green-safe, yellow-prepare for replacement, red-replace the cartridge) or done by time of use. The replacement can even be done by a child, no need to call factory trained personnel for such a change. There is no electricity or battery required, so can be used anywhere, even under load shading.
  • CNS isolated from the pyrolytic combustion of coconut shells was treated with 50% nitric acid and 50% water mixture to introduce carboxylic acid groups due to oxidation which was evident by viewing a lot of brown fumes generated in the process showing reduction of the nitric acid.
  • 1 to 8 hours giving more or less carboxylation
  • varied density number per unit of CNS
  • This first time derivatized CNS (derivatized CNS1) in water under sonication was mixed with an aqueous solution of ferric salt and/or aluminum salt of varied proportion, followed by addition of ammonia to obtain a precipitate (in the pH range 7-8) to rid the mixture of the non metallic part of the salt.
  • Appropriate mixing of the nanospheres with different derivations is done under stirring.
  • the resultant lump is crushed and heated to 100° C. to set silicate or cement to obtain the carbon nano composite.
  • FIG. 1 is a graph of carboxylated concentric carbon nanospheres of the present invention showing D and G band with mixing of overtones around 2700 cm ⁇ 1 in Raman spectrum.
  • FIG. 2 is a chart of EDX of Carboxylated concentric carbon nanospheres of the present invention which shows the presence of oxygen and carbon.
  • FIG. 3 is a SEM image of purified concentric carbon nanospheres of the present invention.
  • FIG. 4 is a TEM image of the purified nanospheres depicted in FIG. 3 .
  • FIG. 5 shows a HRTEM image of the same purified concentric carbon nanospheres which shows their size is in the about 25 nm to about 50 nm range.
  • FIG. 6 shows a SEM image of the present invention carboxylated carbon nanosphere.
  • FIG. 7 shows a SEM image of metallated concentric carbon nanospheres of the present invention.
  • FIG. 8 is a graphic representation of the three types of concentric carbon nanospheres in cross section depicting the concentric spheres.
  • carbon nanospheres are carboxylated to produce carboxylated carbon nanospheres and then metallated to produce metallated carbon nanospheres.

Abstract

The present invention relates to a filter for filtering water comprising carbon nanospheres from the pyrolytic combustion of a carbonaceous material such as plant material which are activated with silver nitrate, activated alumina and/or ferrous oxide.

Description

  • This application is a continuation-in-part of application Ser. No. 13/181,855 filed on Jul. 13, 2011 which claims priority of U.S. provisional application No. 61/365,031 filed on Jul. 16, 2010 and are included herein in their entirety by reference.
  • COPYRIGHT NOTICE
  • A portion of the disclosure of this patent contains material that is subject to copyright protection. The copyright owner has no objection to the reproduction by anyone of the patent document or the patent disclosure as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyright rights whatsoever.
  • BACKGROUND OF THE INVENTION
  • 1. Field of the Invention
  • The present invention relates to the production of carbon nanospheres and to use of the nanospheres in water filters and methods of filtering water using the composition in a water filter device.
  • 2. Description of Related Art
  • Anthropogenic activities have caused severe changes in the natural state of resources in the environment. Essential resources like water and air became unfit for human consumption through pollution. Furthermore, uncontrolled tapping of aquifer for drinking water and its excessive misuse release dormant arsenic or fluoride ion into groundwater finally contaminating surface water and creating potentially serious environmental problems for humans and other living organisms trying to find clean drinking water. Further, pesticides and herbicides accumulate in soil and leach into ground water and water runoff. This is even further aggravated by uncontrolled dumping of used electronic gadgets and batteries in soil. Furthermore, through leakage of water pipes, drinking water contamination with the open sewerage system becomes infected with feces containing pathogenic microbes. Such contaminations are a health risk and there is an urgent demand for a highly effective, reliable, and economical technique for the removal of toxic elements and pathogens from drinking water.
  • A number of methods have been developed to filter or otherwise remove pollutants and unwanted elements from drinking water. Included are methods of precipitation, ceramic or other filters, calcium or magnesium hydroxide, activated carbon, nano silver, chemical reaction, and the like. These materials are frequently used for incorporation as filter material in a filter device such as a housing containing filter material where water can be passed through for filtration purposes. The size of the particle filtered out is directly related to the porosity of the filtering material. Filtration of water is typically divided into nano porous, meso porous, micro porous, and the like.
  • While these methods and materials each have their benefits, they all tend to be limited in what they will filter, in some cases there have been negative health implications and/or high cost and use issues that do not make them the most ideal candidate for purifying drinking water.
  • BRIEF SUMMARY OF THE INVENTION
  • The present invention provides novel filtration material that is cost effective and environmentally friendly, and filtration devices made from those materials. The materials are porous materials that can be used in water filtration devices and to filter other liquids. The porous nanospheres, the nanospheres with carboxyl groups and/or with metallated carboxy groups, can each together or separate be effective in not only filtering water for particulate matter, but in the case of the metallated nanospheres, binding and thus removing arsenic and fluoride and other materials from water passed through such filter material. This combined with ferrice oxide or alumina impregnated with ferric oxide overcomes many of the prior art problems with water filtration.
  • Accordingly, in one embodiment the present invention relates to a water filtering device comprising:
      • a) a first layer of carboxylated activated carbon impregnated with silver;
      • b) a second layer of at least one of activated alumina, activated alumina impregnated with ferric oxide and ferric oxide;
      • c) wherein the layers are arranged such that water passing through the filter passes through the first and second layer.
    BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1 depicts water soluble carbon nanospheres (CNSs) showing D and G band with mixing of overtones around 2700 cm−1 in Raman Spectrum.
  • FIG. 2 is an EDX spectra of CNSs showing the presence of only carbon and oxygen.
  • FIG. 3 is a SEM Image of pure Carbon Nanospheres.
  • FIG. 4 is a TEM image of Carbon Nanospheres.
  • FIG. 5 is a HRTEM image of CNSs showing sizes of the nanospheres with onion type multilayered concentric nanospheres.
  • FIG. 6 is a SEM image of the carboxylated CNSs showing size and shape.
  • FIG. 7 is a SEM image of carboxy metallated CNSs showing sizes of the nanospheres.
  • FIG. 8 is a pictorial representation of the metallation of carboxylated carbon nanosphere.
  • FIG. 9 is a representation of a filter of the present invention.
  • FIG. 10 is a representation of an alternate embodiment of a filter of the present invention.
  • FIG. 11 is a relationship drawing of a microcontroller with filters of the present invention.
  • DETAILED DESCRIPTION OF THE INVENTION
  • While this invention is susceptible to embodiment in many different forms, there is shown in the drawings and will herein be described in detail specific embodiments, with the understanding that the present disclosure of such embodiments is to be considered as an example of the principles and not intended to limit the invention to the specific embodiments shown and described. In the description below, like reference numerals are used to describe the same, similar or corresponding parts in the several views of the drawings. This detailed description defines the meaning of the terms used herein and specifically describes embodiments in order for those skilled in the art to practice the invention.
  • Definitions
  • The terms “a” or “an”, as used herein, are defined as one or as more than one. The term “plurality”, as used herein, is defined as two or as more than two. The term “another”, as used herein, is defined as at least a second or more. The terms “including” and/or “having”, as used herein, are defined as comprising (i.e., open language). The term “coupled”, as used herein, is defined as connected, although not necessarily directly, and not necessarily mechanically.
  • Reference throughout this document to “one embodiment”, “certain embodiments”, and “an embodiment” or similar terms means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, the appearances of such phrases or in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments without limitation.
  • The term “or” as used herein is to be interpreted as an inclusive or meaning any one or any combination. Therefore, “A, B or C” means any of the following: “A; B; C; A and B; A and C; B and C; A, B and C”. An exception to this definition will occur only when a combination of elements, functions, steps or acts are in some way inherently mutually exclusive.
  • The term “about” means±10% unless noted otherwise.
  • The drawings featured in the figures are for the purpose of illustrating certain convenient embodiments of the present invention, and are not to be considered as limitation thereto. Term “means” preceding a present participle of an operation indicates a desired function for which there is one or more embodiments, i.e., one or more methods, devices, or apparatuses for achieving the desired function and that one skilled in the art could select from these or their equivalent in view of the disclosure herein and use of the term “means” is not intended to be limiting.
  • As used herein the terms and phrases “filtration”, “filtration of water”, “water filtering device” and “water filter” refer to material/devices that can be utilized to filter a liquid such as water and remove certain contaminants. The material can be placed/positioned in a filtration device such as a water filter and liquid passed through one or more layers of the filtration material in the normal manner for water filtration. The material can be shaped, placed, containerized, or the like as needed to filter water under gravity pressure or other forced pressure. In other embodiments, liquids other than water that are compatible with carbon filtration material can also be filtered.
  • As used herein the term “nanospheres” refers to concentric spherical carbon structures, granules and the like which outermost spheres are in the size range of about 25 nm to about 50 nm that are isolated from the pyrolytic combustion of a carbonaceous material. The pyrolytic combustion produces concentric spheres that are two or more spheres inside another (see FIG. 8). When collected in a container in quantity (such as being placed in a filter), the nanospheres fill a given space like marbles fill a container, creating the minimal amount of space possible and aligning themselves due to their spherical shape. The porosity of the material is derived by spaces in-between the spheres since there is a consistent size of that space when packing spherical objects. The space between the spheres can be adjusted, that is, made smaller, thus filtering smaller particles by placing addition groups on the surface of the spheres, thus making them fuzzy and thus taking up space in the space between the spheres. The present invention includes carboxylation of the spheres wherein carboxylation is obtained by oxidation of the spheres. Greater carboxylation of the spheres requires the spheres to remain in contact with the oxidizing agent (such as nitric acid) for a longer period. The carboxylation, once it reaches a certain point, makes the spheres water soluble, therefore, in the case where they are to be utilized for water filtration, the carboxylation should be kept below an amount that makes them soluble in the water being filtered. That amount can easily be determined by varying the oxidation time and testing a batch. Where a fluid other than water is being filtered, the amount of carboxylation can be less important.
  • The carboxylate groups can also be metallated. Metallation will cause the spheres to be non-water soluble so, in that instance as much carboxylation as desired can be done. One can combine these additions to the spheres having all carboxylation or metallization on a sphere, a combination of the two on a sphere, or a combination of spheres that are each all carboxylated or metallated. The non substituted spheres and these substituted spheres can be mixed together in any combination desired depending on the porosity desired. The more substitutions, the smaller the spaces and the smaller the particle that is filtered out by the material.
  • In general, the material is loosely packed and can be placed in a cartridge or other container to hold it in place during the filtration process. In other embodiments, a binder can be utilized to make the spheres sticky enough to hold together as a composite. For example, a silicic acid solution could coat the spheres without decreasing significantly the porosity of the material. Other binders, such as low density polyethylene or ethyl vinyl acetate, could be determined by one skilled in the art.
  • As used herein the phrase “not carboxylated sufficiently to cause the carbon nano spheres to be water soluble” refers to only oxidizing the spheres enough so that the resulting spheres are still not soluble in water to a significant degree.
  • As used herein the terms “metal ion”, “metallate”, “metallation”, and “metallated” refer to treating the carboxylate groups' place on the nanospheres to place a metal ion on the group in place of the carboxylic group, i.e. replacing —COON with —COM wherein M is the metal ion. Metal ions can be selected from metals in the transition metals and poor metal groups from the periodic table. For example, iron, silver, and aluminum could be selected. The ions can be delivered in the form of the ion or a salt which dissociates to deliver the metal ion. It is known that certain ions can bind compounds and the selection of the metal ion can be done to selectively bind certain compounds dissolved in the liquid such as water in addition to filtering the media. For example, in some cases silver is known to attach to bacteria binding it, and in other cases actually killing it. Iron and aluminum can bind arsenic and fluoride respectively and can similarly be utilized. One skilled in the art can determine which metal to select based on binding capacity, cost, ease of use, and the like.
  • As used herein a “carbonaceous material” refers to material which when pyrolyzed, can form carbonaceous nanospheres (about 25 nm to about 50 nm in size). In one embodiment, the carbonaceous material is an organic material that is a material that was living such as animal or plant material. For example, the material could be a cellulosic material, wood, coconut shell, wood wool, wood dust, or the like. Other materials can also be utilized which can be pyrolyzed in sufficient quantity to make enough spheres to make a filter.
  • As used herein, “oxidizing agent” refers to a composition that can oxidize the surface of a carbon sphere to produce carboxylic acid groups on the surface, for example concentrated or diluted nitric acid; though there is damage to the spheres the more concentrated the acid is.
  • As used herein, “activated carbon with silver nitrate” refers to carbon granules which have adsorbed onto it silver nitrate for the purpose of inhibiting growth of bacteria. In order to achieve this, for example, 0.2 milligrams of silver nitrate is dissolved in one liter of “distilled water” to prepare a 2 ppm (parts per million) solution. About 2 kilograms of carboxylated activated carbon granules are soaked in the 2 ppm silver nitrate solution for 1-2 hours. This soaked mass is dried in sun rays and then heated to 180° C. which results in impregnating the activated carbon with metallic silver. Silver nitrate is photo decomposed and finally thermally decomposed and metallic silver is impregnated to the entire mass of the nano carbon carboxylate. This carboxylated activated carbon impregnated with silver in this form prevents/retards any bacteria biofilm formation.
  • As used herein, “activated alumina” is aluminum hydroxide made by dehydroxylating it in a way that produces a highly porous material. In order to activate it with ferric oxide, 10% (of alumina weight) ferrous sulphate solution, in 50-150 mL water, is added to alumina granules (size 0.5-2 mm) and mixed well gently. 10% ammonia solution is added until the pH of the supernatant becomes 6-7. The alumina granules turn green. These green granules are left in the air and shaken well for auto-oxidation in atmospheric air. As a result, the green colored granules turn an orange-red color. These air-dried, orange-red alumina granules are heated up to and kept at 400° C. in a furnace for 1 hour. Then the furnace is allowed to cool at room temperature. Now the orange-red alumina is ready to be used as an adsorbent for fluoride and arsenic present in the water.
  • In one embodiment, the filter can be combined with a microcontroller. The microcontroller can control if water passes through the filter or if the filter needs changing. So, for example, if a filter needs changing, the filter could be shut off. In another embodiment, the filter is digitally identified by the microcontroller so once the filter is used up, the microcontroller will never let it be used again preventing reuse of spent filters or use beyond useful life.
  • Preparation of Nanospheres
  • Concentric carbon nanospheres (CNS) are prepared by the pyrolysis of carbonaceous material under insufficient air. The carbonaceous material can be any material capable of pyrolysis (600 to 850° C.) that produces nanospheres but in one embodiment is a natural material such as a biologic animal or plant material. Examples include but are not limited to coconut shell, wood wool, and wood dust. It can also include cellulose materials and wood.
  • In one embodiment, fire/heat is applied to the carbonaceous material in a confined chamber under the flow of blowing air where the carbonaceous matter is allowed to glow. An outlet on the top of the chamber continuously ejects the distillation byproducts such as ligneous acid under the flow of air from the bottom of the chamber maintained at a temperature around 600-850° C. The process takes several hours and is dependent on the quantity of the feed stock. When the oily byproduct ceases to come out through the top outlet, water is slowly introduced by sprinkling and the steam produced is dispersed or removed along with the residual byproduct. The residual mass is also cooled down. The mass is leached with alcohol to remove traces of soluble organic byproduct, especially products like ligneous acid which can be trapped in the pores (spaces between the spheres) and air dried. It can also be washed with 10% sodium hydroxide solution for that purpose. The dried mass is pulverized to get the desired size of pieces containing multiple carbon nano spheres (macro sized, in the millimeter range) by using appropriate mesh size while the individual spheres are together as shown in the SEM photographs. The CNS is now ready for further derivitization processes like carboxylation followed by metallation or can be utilized as is as a filtration material.
  • The collected black material from pyrolysis of the carbonaceous material which comprises amorphous carbon and carbon nanospheres is purified by washing. In one embodiment, ligneous acid and other impurities are removed by washing with a solution of 10% sodium hydroxide. This can then be subjected to a first derivitization by treating it with an oxidizing agent such as nitric acid to introduce multiple carboxylic acid groups on the surfaces of the CNS. The longer the spheres are oxidized, the greater the carboxylization. The carboxylated derivatized CNS are treated under sonication in water and are subjected to a second derivitization by adding metal ions such as ferric ion and aluminum ion and by adjusting the pH to metallate at least a portion of the carboxylic acid groups. The formation can occur with the addition of ammonia followed by drying the mixture to a dried residue. Appropriate mixing and drying is done at each step. In most cases, what remains is a combination of spheres that are carboxylated, some that are metallated or a combination of the two. Non-deritivized spheres may remain as well. As noted, the filter material can contain any combination of the three types of nanospheres either because they all exist during producing them or because they are made separately and combined. The concentration of metal to CNS can vary from about 0.2% to about 10% by weight (of total CNS weight). The resultant mass is washed with water to remove free metal ions and other counter ions and heated to around 100° C. to yield the metal impregnated form of CNS. See FIG. 8 for example. All these forms are activated carbon with assorted porosity.
  • Creating a Filter
  • The material of the present invention can then be placed in a container or otherwise contained or formed as necessary for the desired filtration purpose or filter or filter holder. The shape can be as needed, for example to be placed in the flow of water to be filtered either by gravity or pressure filtration. For example, it can be contained in a standard filter holder or the like or custom holders for inline use can be created and such are unlimited in variety and shape. For example, where under gravity, thinner filters can be utilized, up to 8 inches, depending on how much must be filtered out. In the case of high pressure filtration, virtually any thickness can be utilized as long as the pressure is not so great as to damage the filter material of the present invention. When CNS are prepared from low cost material, it can be utilized to develop eco-friendly filters that trap or bind soluble compounds of toxic metal ions and anions, pathogens and virus, and industrial organic molecules like pesticides and aromatic hydrocarbons as well as color and odor in a unique integrated manner. The filter material of the present invention is also capable of reducing the salinity of water. The advantage of this invention over the comparable inventions lies on the following: the proposed system can remove inorganic, organic and bio related toxic materials commonly available in water to make the water safe for drinking purposes. The proposed system also requires no energy input as normally needed in systems that use ozone, ultraviolet radiation, chlorination, or reverse osmosis to remove pathogens and virus. The composition traps these pathogens in the pores and surface of CNS without need for any energy input.
  • The filter material which has bound materials such as arsenic and fluoride and bacteria to it can be chemically treated to regenerate the material. However, because of the low cost involved in the manufacturing of the material, it can be readily disposed of or used as crude carbonaceous fuel if it no longer filters sufficiently for filtration utilization.
  • Preparation of Water Filter Cartridges (Alumina, Ferric Oxide & Carbon) Using Polypropylene or Polyethylene As Binders
  • In this embodiment silver impregnated nano carbon granules with either ferric oxide impregnated alumina globules or ferric oxide globules or both, are added with 5-10% of the binder such as polypropylene or polyethylene (high or low density) powder. These are mixed thoroughly and placed in cylindrical shaped molds. Pressure is applied to the top surface of the mixed powder in the mold along with application of heat to the metallic mold in order to bring the temperature up to the melting point of the organic binder (i.e polypropylene, polyethylene or any other binder). After a few minutes, the heating is stopped to allow the composite material to shrink/contract. After a couple of hours, when the mold is cooled off, the cylindrical cartridge which is now in solid form is removed and is ready for use as a filter.
  • In other embodiments, the silver impregnated nano carbon with ferric oxide coated alumina in a particular ratio depending on the level of fluoride or arsenic in the water in a specific area. Cylindrical shape of this composite mixture is created as described above. In select areas where water contains predominantly fluoride, the alumina globules will be used along with the silver impregnated nano carbon granules. In areas where water contains predominantly Arsenic, then ferric oxide globules activated by heating to about 400° C., will be used along with the silver impregnated nano carbon granules. In areas where fluoride is prominent but arsenic is in traces, then alumina treated with nano ferric oxide along with silver impregnated nano carbon granules will be used. When both arsenic and fluoride are present in water, then alumina globules and ferric oxide globules will be used proportionately depending on which (arsenic or alumina) has higher content. Silver impregnated nano carbon granules will be used as well.
  • The relative variation in ratios of the silver impregnated nano carbon to ferric coated alumina and ferric oxide globules will provide varied version of filter cartridges dependent on the need based on the quality of water. If just (a) organic molecules such as petroleum products, pesticides, herbicides (b) microbes, pathogenic coli, viruses and (c) heavy metals like mercury or cadmium or lead are present in the water, then the activated nano carbon alone is effective. If the water is contaminated with fluoride as well, then a proportionate amount of ferric treated alumina is required in the cartridges. Similarly, if water is contaminated with arsenic as well, then a proportionate amount of ferric oxide granules is included along with the silver impregnated carbon in the hybrid filtration cartridge. Filter material binded with the help of binders such as polypropylene and polyethylene increase the contact time of water as it passes through the cylindrical wall of the compressed hybrid carbon nano filter. This enhances the performance of filtration compared with filter material in the loose granular format.
  • In one embodiment seen in FIG. 9, the filter 1 consists of the following horizontal layers. Unfiltered water enters the top 2 of the filter 1 and encounters the top most layer 5 of the filter which consists of silver impregnated carbon nano. Next, the pesticides middle layer 4 consists of activated alumina treated with ferric oxide, activated alumina globules, or ferric oxide globules, depending on the presence of fluoride and or arsenic and their levels in water to be filtered. The last layer 3 consists of Calcium Bentonite and Somelite to remove any traces of bacteria, toxins and heavy metals. In addition, this last layer helps to enhance the taste of water. Finally, filtered water 6 is removed from the bottom of the filter.
  • The filter may be of any convenient size. The treated carbon material and ferric oxide impregnated alumina or ferric oxide globule may be separately placed in different partitions (this is done to get the carbon regenerated readily after use). In one embodiment, it may work as follows:
  • Unfiltered water enters through the top for filtration. Strainers hold carbon and alumina in respective chambers. Filter material is held in place with screw filters (carbon and alumina, respectively). Water enters a port for water entry into the filtration chambers with an additional particulate chamber (step 1) to trap suspended particulates. A valve is present to regulate flow. A device for creating backflow is included for flushing purposes. After passing through both filters, water is stored in a small reservoir. Filtered water exits through an appropriate valve if deserved.
    This gravity type filter needs no power to operate—runs using force of gravity. It also uses nano carbon and nano silver, nano ferric oxide, and nano alumina to trap all biological, organic and inorganic toxic materials. It does not require a high level of skill to operate, no mechanical parts that wear out and require replacement, and it has simple plumbing when compared to regular type systems. The carbon and alumina can be regenerated and reused (recycling). The filter removes bacteria as well as fluoride and arsenic (more fluoride removal than a conventional system).
  • When making a small version of the gravity filter, once used, the cartridge can be discarded, and depending on the need of cartridge, one can use only carbon or carbon with alumina treated with ferric oxide or carbon with ferric oxide or carbon with both alumina and ferric oxide.
  • A tap filter (one that can attach to a faucet or the like is shown in FIG. 10). The parts and layers have the indicated materials but the water to be filtered 2 enters the center of the filter and is pushed horizontally by the pressure of the flow of water to produce filtered water 6 on the outside of the filter. It also removes bacteria, other toxic organic and biological contaminants, toxic heavy metals as well as fluoride and arsenic (more fluoride removal than conventional system). It is small and portable and requires only overhead tank water pressure operative even on the top most floor of a building. Replacement of cartridges will be indicated with flashing indicator light (green-safe, yellow-prepare for replacement, red-replace the cartridge) or done by time of use. The replacement can even be done by a child, no need to call factory trained personnel for such a change. There is no electricity or battery required, so can be used anywhere, even under load shading.
  • EXAMPLES Example 1
  • CNS isolated from the pyrolytic combustion of coconut shells (by the method above) was treated with 50% nitric acid and 50% water mixture to introduce carboxylic acid groups due to oxidation which was evident by viewing a lot of brown fumes generated in the process showing reduction of the nitric acid. After few hours of standing, 1 to 8 hours (giving more or less carboxylation), varied density (number per unit of CNS) of carboxylation took place. The nitric acid is washed away with plenty of water until the mass is nitrate free and the black slurry is dried in air. This first time derivatized CNS (derivatized CNS1) in water under sonication was mixed with an aqueous solution of ferric salt and/or aluminum salt of varied proportion, followed by addition of ammonia to obtain a precipitate (in the pH range 7-8) to rid the mixture of the non metallic part of the salt. This was treated with plenty of water to remove the water soluble ions and dried in air to obtain a dried residue as second time derivatized CNS. Appropriate mixing of the nanospheres with different derivations is done under stirring. The resultant lump is crushed and heated to 100° C. to set silicate or cement to obtain the carbon nano composite.
  • Example 2
  • 1 mm sized globular alumina was treated with 10% aqueous solution of ferrous sulfate and allowed to soak for couple of hours. The slurry was made ammoniacal by adding 5% aqueous solution of ammonia whereby greenish black ferrous oxide precipitated out and adhered to the alumina surface. This material was then air dried whereby green ferrous oxide got oxidized to brown ferric oxide. The iron oxide impregnated alumina was then heated in a muffle furnace at about 380° C. to drive off or remove volatile ammonium sulfate and water and activate the material (iron oxide impregnated alumina) which can now be used for removal of fluoride ions during filtration of water.
  • Example 3
  • A protocol with reasonable rate of water flow is described here. 50 grams of the activated alumina impregnated with iron oxide was used to test its capacity to bind fluoride. Water containing 4 ppm (parts per million) level of fluoride ion was filtered at the rate of 5 liter of water per hour for the first stage of 100 liters of water. This was followed by 2 ppm level of fluoride for another 350 liters of water. The result was that 1.1 gm of fluoride was removed in this manner by using 50 gm of activated alumina impregnated with iron oxide filter bed. The flow rate is adjusted by using normal force of gravity without any external energy input source.
  • Example 4
  • 100 grams of activated alumina impregnated with iron oxide (filter bed) and 53 liters of water containing 4 ppm fluoride (4 ppm means 12 mgs of potassium fluoride per liter of water) is used at initial stage of filtration. In the next stage, 113 liters of water containing 2 ppm of fluoride (6 mgs of potassium fluoride per liter of water) is passed through the filter bed. It is shown that removal of fluoride is 2.2 gm measured as potassium fluoride.
  • Example 5
  • Similarly, using 50 gm of the modified ignited alumina impregnated with iron oxide as filter bed, water containing 5 ppm level of arsenic was passed through this bed at a flow rate of 5 liter of water per hour, and measured grams of arsenic were removed from a passage of a quantity of water.
  • EXPLANATIONS OF THE DRAWINGS AND FIGURES
  • FIG. 1 is a graph of carboxylated concentric carbon nanospheres of the present invention showing D and G band with mixing of overtones around 2700 cm−1 in Raman spectrum.
  • FIG. 2 is a chart of EDX of Carboxylated concentric carbon nanospheres of the present invention which shows the presence of oxygen and carbon.
  • FIG. 3 is a SEM image of purified concentric carbon nanospheres of the present invention.
  • FIG. 4 is a TEM image of the purified nanospheres depicted in FIG. 3.
  • FIG. 5 shows a HRTEM image of the same purified concentric carbon nanospheres which shows their size is in the about 25 nm to about 50 nm range.
  • FIG. 6 shows a SEM image of the present invention carboxylated carbon nanosphere.
  • FIG. 7 shows a SEM image of metallated concentric carbon nanospheres of the present invention.
  • FIG. 8 is a graphic representation of the three types of concentric carbon nanospheres in cross section depicting the concentric spheres. In each sphere, carbon nanospheres are carboxylated to produce carboxylated carbon nanospheres and then metallated to produce metallated carbon nanospheres.
  • Those skilled in the art to which the present invention pertains may make modifications resulting in other embodiments employing principles of the present invention without departing from its spirit or characteristics, particularly upon considering the foregoing teachings. Accordingly, the described embodiments are to be considered in all respects only as illustrative, and not restrictive, and the scope of the present invention is, therefore, indicated by the appended claims rather than by the foregoing description or drawings. Consequently, while the present invention has been described with reference to particular embodiments, modifications of structure, sequence, materials and the like apparent to those skilled in the art still fall within the scope of the invention as claimed by the applicant.

Claims (9)

What is claimed:
1. A water filtering device comprising:
a) a first layer of carboxylated activated carbon impregnated with silver;
b) a second layer of at least one of activated alumina, activated alumina impregnated with ferric oxide and ferric oxide;
c) wherein the layers are arranged such that water passing through the filter passes through the first and second layer.
2. The water filtering device according to claim 1 further comprising a third later of at least one of somelite and bentonite.
3. The water filtering device according to claim 1 wherein the filter material of the layers are held together with a binder.
4. The water filtering device according to claim 3 wherein the binder is selected from the group consisting of silica, polypropylene and polyethylene.
5. The water filtering device according to claim 1 which is a gravity water filter.
6. The water filtering device according to claim 1 which is a tap water filter.
7. Ferric oxide activated alumina.
8. The water filter device according to claim 1 which is further combined with a microcontroller which controls the filter use.
9. The water filter according to claim 8 wherein the microcontroller controls at least one of passage of water through the filter and when to change the filter.
US13/791,058 2010-07-16 2013-03-08 Water filtration system using hybrid nano carbon, silver, iron and aluminium oxide Abandoned US20130180913A1 (en)

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US13/181,855 US20120012522A1 (en) 2010-07-16 2011-07-13 Making and using composite material containing nanospheres and devices for water filtration and devices containg such composites
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US9833747B2 (en) * 2015-12-30 2017-12-05 Sangmyung University Industry-Academy Cooperation Foundation Polymer electrolyte membrane containing nitrate for sulfur hexafluoride separation
CN109293035A (en) * 2018-11-30 2019-02-01 庄再聪 A kind of Portable water purifier
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WO2021256946A1 (en) * 2020-06-17 2021-12-23 Qatar Foundation For Education, Science And Community Development Activated carbon-composite materials, filters, and preparation methods thereof

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